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In the title compound, (NH4)[ZnCl3(C6H12N4)]·1.5H2O, the ZnII atom is in a tetra­hedral environment, coordinated by one N atom of the hexa­methyl­enetetra­mine ligand and by three Cl atoms. The charge of the hexa­methyl­enetetra­mine­trichloro­zincate(II) anion is counter-balanced by an ammonium cation. Two water mol­ecules, one of which shows disorder and is only partly occupied, are also present. The structure is stabilized by weak inter­molecular O—H...N, N—H...O and N—H...N hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806050550/wm2072sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806050550/wm2072Isup2.hkl
Contains datablock I

CCDC reference: 630498

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](N-C) = 0.004 Å
  • H-atom completeness 95%
  • Disorder in main residue
  • R factor = 0.040
  • wR factor = 0.093
  • Data-to-parameter ratio = 16.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O2 PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O2' PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. O2 .. 3.26 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1A .. CL1 .. 2.87 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H5A .. CL2 .. 2.90 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H6A .. CL2 .. 2.86 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 0.83(4), Rep 0.823(18) ...... 2.22 su-Ra O1 -H1WA 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Ra O1 -H1WB 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.83(4), Rep 0.823(18) ...... 2.22 su-Ra O1 -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Ra O1 -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Ra O1 -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Ra O1 -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.842(19) ...... 2.11 su-Ra O1 -H2# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.01(4), Rep 2.012(19) ...... 2.11 su-Ra H1# -N4 1.555 1.555
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C6 H19 Cl3 N5 O1.5 Zn1 Atom count from the _atom_site data: C6 H18 Cl3 N5 O1.5 Zn1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C6 H19 Cl3 N5 O1.50 Zn TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 24.00 24.00 0.00 H 76.00 72.00 4.00 Cl 12.00 12.00 0.00 N 20.00 20.00 0.00 O 6.00 6.00 0.00 Zn 4.00 4.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 13 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SMART; data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXTL (Bruker, 2002); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Ammonium trichloro(hexamethylenetetramine)zincate 1.5-hydrate top
Crystal data top
(NH4)[ZnCl3(C6H12N4)]·1.5H2OF(000) = 728
Mr = 357.96Dx = 1.650 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3136 reflections
a = 8.7692 (19) Åθ = 2.3–27.0°
b = 9.621 (2) ŵ = 2.26 mm1
c = 17.137 (4) ÅT = 273 K
β = 94.842 (4)°Block, colourless
V = 1440.6 (5) Å30.37 × 0.35 × 0.32 mm
Z = 4
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3136 independent reflections
Radiation source: fine-focus sealed tube2694 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
φ and ω scansθmax = 27.0°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 119
Tmin = 0.444, Tmax = 0.499k = 812
8538 measured reflectionsl = 1821
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0367P)2 + 0.9695P]
where P = (Fo2 + 2Fc2)/3
3136 reflections(Δ/σ)max = 0.001
187 parametersΔρmax = 0.33 e Å3
3 restraintsΔρmin = 0.35 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn10.64545 (3)0.04267 (3)0.83373 (2)0.03070 (12)
Cl10.69797 (10)0.04665 (9)0.70755 (5)0.0479 (2)
Cl20.72682 (9)0.15574 (8)0.89069 (5)0.0429 (2)
Cl30.73478 (10)0.23086 (10)0.90084 (6)0.0576 (3)
O10.1794 (3)0.4063 (3)0.97510 (14)0.0424 (5)
N50.0184 (3)0.6316 (3)0.89970 (17)0.0352 (6)
O20.4684 (18)0.511 (2)1.0414 (10)0.078 (4)0.25
O2'0.4768 (19)0.5626 (16)0.9878 (16)0.079 (4)0.25
N10.4053 (2)0.0394 (2)0.83495 (13)0.0243 (5)
N20.1795 (3)0.0946 (2)0.86587 (15)0.0317 (5)
N30.1616 (3)0.0665 (3)0.75544 (14)0.0341 (6)
N40.1887 (3)0.1553 (2)0.88907 (14)0.0321 (5)
C10.3468 (3)0.0951 (3)0.86481 (17)0.0311 (6)
H1A0.37670.17050.83180.037*
H1B0.39310.11150.91740.037*
C20.1113 (3)0.0675 (3)0.78613 (18)0.0358 (7)
H2A0.00070.06740.78620.043*
H2B0.13950.14170.75180.043*
C30.1198 (3)0.1767 (3)0.80870 (19)0.0376 (7)
H3A0.00930.17970.80910.045*
H3B0.15320.26560.78950.045*
C40.3553 (3)0.1522 (3)0.88707 (17)0.0297 (6)
H4A0.40250.13800.93970.036*
H4B0.38980.24120.86860.036*
C50.3289 (3)0.0635 (3)0.75469 (17)0.0331 (6)
H5A0.36380.15110.73450.040*
H5B0.35770.01000.72000.040*
C60.1358 (3)0.0197 (3)0.91692 (17)0.0330 (6)
H6A0.18020.00360.96990.040*
H6B0.02540.02140.91790.040*
H5F0.047 (4)0.638 (4)0.935 (2)0.052 (11)*
H5E0.078 (4)0.567 (4)0.912 (2)0.042 (10)*
H5C0.034 (5)0.611 (4)0.849 (3)0.075 (13)*
H1WA0.178 (5)0.333 (3)0.950 (3)0.11 (2)*
H1WB0.267 (4)0.426 (5)0.997 (3)0.15 (3)*
H5D0.064 (5)0.715 (5)0.891 (3)0.088 (15)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.02226 (18)0.0319 (2)0.0383 (2)0.00374 (13)0.00418 (13)0.00107 (14)
Cl10.0440 (5)0.0569 (5)0.0454 (5)0.0089 (4)0.0193 (4)0.0106 (4)
Cl20.0416 (4)0.0394 (4)0.0460 (4)0.0145 (3)0.0051 (3)0.0039 (3)
Cl30.0395 (5)0.0479 (5)0.0851 (7)0.0072 (4)0.0043 (4)0.0217 (5)
O10.0507 (15)0.0371 (13)0.0405 (13)0.0130 (11)0.0104 (11)0.0021 (10)
N50.0349 (15)0.0373 (16)0.0339 (15)0.0104 (13)0.0057 (12)0.0075 (12)
O20.085 (10)0.072 (10)0.073 (11)0.013 (9)0.019 (8)0.023 (11)
O2'0.071 (9)0.082 (11)0.079 (12)0.001 (8)0.013 (8)0.027 (11)
N10.0208 (11)0.0245 (12)0.0277 (11)0.0008 (9)0.0026 (9)0.0002 (9)
N20.0244 (12)0.0294 (12)0.0414 (14)0.0029 (10)0.0038 (10)0.0020 (11)
N30.0230 (12)0.0462 (15)0.0325 (13)0.0001 (10)0.0014 (10)0.0042 (11)
N40.0214 (11)0.0328 (13)0.0426 (14)0.0015 (10)0.0048 (10)0.0070 (11)
C10.0294 (14)0.0244 (14)0.0395 (16)0.0012 (11)0.0026 (12)0.0040 (12)
C20.0266 (14)0.0386 (17)0.0417 (17)0.0054 (12)0.0007 (12)0.0085 (13)
C30.0237 (14)0.0339 (16)0.0549 (19)0.0052 (12)0.0019 (13)0.0081 (14)
C40.0219 (13)0.0297 (15)0.0375 (15)0.0013 (11)0.0016 (11)0.0064 (12)
C50.0250 (14)0.0459 (18)0.0281 (14)0.0007 (12)0.0016 (11)0.0034 (12)
C60.0259 (14)0.0408 (17)0.0328 (15)0.0013 (12)0.0052 (11)0.0010 (13)
Geometric parameters (Å, º) top
Zn1—N12.108 (2)N3—C31.466 (4)
Zn1—Cl22.2335 (9)N3—C51.469 (3)
Zn1—Cl12.2487 (10)N3—C21.474 (4)
Zn1—Cl32.2500 (10)N4—C41.464 (3)
O1—H1WA0.823 (18)N4—C31.471 (4)
O1—H1WB0.842 (19)N4—C61.477 (4)
N5—H5F0.87 (4)C1—H1A0.9700
N5—H5E0.82 (4)C1—H1B0.9700
N5—H5C0.97 (4)C2—H2A0.9700
N5—H5D0.92 (5)C2—H2B0.9700
O2—O2i1.58 (3)C3—H3A0.9700
O2'—O2'i1.33 (3)C3—H3B0.9700
N1—C41.494 (3)C4—H4A0.9700
N1—C51.496 (3)C4—H4B0.9700
N1—C11.498 (3)C5—H5A0.9700
N2—C21.468 (4)C5—H5B0.9700
N2—C11.469 (3)C6—H6A0.9700
N2—C61.476 (4)C6—H6B0.9700
N1—Zn1—Cl2105.41 (6)N1—C1—H1B109.2
N1—Zn1—Cl1107.20 (6)H1A—C1—H1B107.9
Cl2—Zn1—Cl1110.54 (3)N2—C2—N3112.2 (2)
N1—Zn1—Cl3108.17 (6)N2—C2—H2A109.2
Cl2—Zn1—Cl3112.32 (4)N3—C2—H2A109.2
Cl1—Zn1—Cl3112.77 (4)N2—C2—H2B109.2
H1WA—O1—H1WB113 (3)N3—C2—H2B109.2
H5F—N5—H5E109 (3)H2A—C2—H2B107.9
H5F—N5—H5C110 (3)N3—C3—N4112.1 (2)
H5E—N5—H5C108 (3)N3—C3—H3A109.2
H5F—N5—H5D112 (4)N4—C3—H3A109.2
H5E—N5—H5D115 (3)N3—C3—H3B109.2
H5C—N5—H5D103 (4)N4—C3—H3B109.2
C4—N1—C5107.8 (2)H3A—C3—H3B107.9
C4—N1—C1107.3 (2)N4—C4—N1111.8 (2)
C5—N1—C1107.9 (2)N4—C4—H4A109.2
C4—N1—Zn1109.81 (15)N1—C4—H4A109.2
C5—N1—Zn1111.01 (16)N4—C4—H4B109.2
C1—N1—Zn1112.80 (15)N1—C4—H4B109.2
C2—N2—C1108.5 (2)H4A—C4—H4B107.9
C2—N2—C6108.3 (2)N3—C5—N1111.4 (2)
C1—N2—C6108.6 (2)N3—C5—H5A109.3
C3—N3—C5108.8 (2)N1—C5—H5A109.3
C3—N3—C2108.2 (2)N3—C5—H5B109.3
C5—N3—C2108.4 (2)N1—C5—H5B109.3
C4—N4—C3108.2 (2)H5A—C5—H5B108.0
C4—N4—C6109.4 (2)N2—C6—N4111.2 (2)
C3—N4—C6108.1 (2)N2—C6—H6A109.4
N2—C1—N1111.9 (2)N4—C6—H6A109.4
N2—C1—H1A109.2N2—C6—H6B109.4
N1—C1—H1A109.2N4—C6—H6B109.4
N2—C1—H1B109.2H6A—C6—H6B108.0
Symmetry code: (i) x+1, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1WA···N40.82 (2)2.01 (2)2.834 (3)176 (3)
O1—H1WB···O20.84 (2)2.04 (2)2.871 (17)169 (3)
O1—H1WB···O20.84 (2)2.28 (2)3.002 (16)144 (3)
O1—H1WB···O2i0.84 (2)2.54 (2)3.225 (17)139 (3)
O1—H1WB···O2i0.84 (2)2.25 (2)3.043 (17)158 (3)
N5—H5E···O10.82 (4)2.05 (4)2.838 (4)160 (3)
N5—H5F···O1ii0.87 (4)2.05 (4)2.894 (4)163
N5—H5C···N3iii0.97 (4)2.08 (4)3.040 (4)176 (3)
N5—H5D···N2iv0.92 (5)2.15 (5)3.067 (4)177 (4)
C1—H1A···Cl1v0.972.873.673 (3)141
C5—H5A···Cl2vi0.972.903.679 (3)138
C6—H6A···Cl2vii0.972.863.655 (3)140
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z+2; (iii) x, y+1/2, z+3/2; (iv) x, y+1, z; (v) x+1, y1/2, z+3/2; (vi) x+1, y+1/2, z+3/2; (vii) x+1, y, z+2.
 

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